Method of producing mgcl2 containing chlorides of alkali metals or alkaline earth metals



Patented Mar. 21, 1933 UNITED STATES PATENTQFFECE HIROSHI TANAKA, OF KOMAGOME,

MAGHI, EBARA-GUN, TOKYO, JAPAN, KENKYUJ'O, OF TOKYO, JAPAN HONGO-KU, AND SHOICHIR'O' IMATOMI, IKEGAMI- ASSIGNORS TO ZAIDAN I-IOJ'IN RIKAGAKU METHOD OF PRODUGIN G MgCl: CONTAINING OHLoRIDEs OF ALKALI METALS OR ALKALINE EARTH METALS No Drawing. Application filed March 8, 1929,

This invention relates to an improvement in a process of producing anhydrous magnesium chloride by passing chlorine gas through magnesium sulphide or magnesium sulphide which contains or is mixed with chlorine gas or a reducing gas containing chlorine gas therethrough. By this process, anhydrous magnesium chloride containing chloride of an alkali metal or of an alkaline earth metal can be producedin melted state at acomparatively low temperature and with good yield.

The melting point of anhydrous pure magnesium chloride is 708 C. and the dife ference between the melting point and its vaporizing point is very small. Therefore, when preparing anhydrous magnesium chloride in melted state by passing chlorine gas through magnesium sulphide or same containing magnesium oxide, there is unavoidable loss of a part of the anhydrous magnesium chloride produced owing to its evaporation.

According to this invention, said drawback is entirely obviated by preparatory mixing one or more chloride or sulphide of alkali metals or of alkaline earth :metals to the raw material, thatis, to magnesium sulphide or the same containing magnesium oxide. When such mixture is treated with chlorine gas or a reducing gas containing chlorine gas under heating, the sulphide of the metal, when this is used, easily becomes the corresponding'chloride and is melted together with magnesium chloride produced.

Serial No. 345,594, and in Japan Apri1'12, 1928.

When chloride of the metal is used, this is directly melted together with magnesium chloride produced. This magnesium chloride containing chloride of alkali metal or alkaline earth metals such as Na, K, Li, Ca, Ba, Sr and the like has a melting point far lower than that of anhydrous pure magnesium chloride while, its boiling point is 7 higher than that of the same. Therefore, a partial loss of anhydrous m gnesium chloride produced can be obviated. Moreover, the mixture of magnesium chloride and chloride of the metal is a very thin fluid in melted state so that the operation of chlorinating is made easier as well as its reaction is fully carried out at a comparatively low temperature. f c

The anhydrous MgGl produced in this process is not separated from thechlorides of alkali metals or alkaline earth metals,

- the object of the invention being to manufacture a mixture of anhydrousMgCl and the other chlorides melted together.

By the new method the melting is carried out at a comparatively low temperature so that the loss of MgCl owing to its vaporization is possibly decreased.

Example I First material: magnesium sulphide containing magnesium oxlde.

Per cent Magnesium sulphide 53. O 7 Magnesium oxide 40. 8 Lime, alumina etc fl. 2 Iron 0.7 Water insoluble part; 1.3

" Second material: pure potassium chloride.

150 grams of thefirst material is mixed with 30 grams of the second material. The mixture is charged in a shaft furnace and is heated to 650 (1, and chlorine gas is passed through. 230 grams of white crystal product flowed down on the lower part of the furnace, and which has the followin composition.

Per cent treatment of the mixture as in the first example, the percentages of the yield are:

Anhydrous magnesium chloride 84.1 A Per cent nhydrous IllfiWIlQSlllIIl chloride 84.0 'Potalsslum1 h 3 Sodium chloride 12. 3 Calcium cnlorlde and others 2. 0 Gale-mm Chlori (1e and Others 2 3 Iron ion jj'jj'j'j' 0'1 Insoluble matter u 4 Water insoluble matter O. 5

' Example [1 Example V First material: Per cent First material:

. Magnesium i l 7 0 Magnesium sulphide f g: d MagneSmm oxlde u 0 Magnesium oxide 40. 8 Lune 7-? 5 Lime alumina etc 4.2 Iron, alummium etc 2.1 Iron 7 Second material: Water insoluble matter 1. 3

' Parts Potassium chloride 1 Second material: P q l chloricle 1 Calcium s111phite; Llthlum "ffj f 1 Composition Sodium chloride 15 45% of second material s m1xed with first P t i hl id 15 material, charged into a shaft furnace which 3 0 mm o Se material is added to o A I I gzg ii gii g 252 2 12222: 22 100 grams of first material, charged into E as p b a shaft furnace, heated to 600 C. and passed PM t through chlorine gas. The percentages of Anhydrous magnesium chloride 7 5.3 the yield are: v P Vt er cen gggi g gfig ifi n Anhydrous magnesium chloride 81. 0 Lithium chloride C f5 Sodium chloride 8 Calcium chloride :j: 1.1 Pomdsium chloride" 9 Water insoluble matter 0.2 g g chlonde and Others b Ewampze 1H Water insoluble matter 0. 5

First material:

?er cent Magnesium sulphide 53. 0

Magnesium oxide 40.0

Lime, alumina etc- 4. 2

Iron 0.7

Water insoluble matter 1. 3 Second material: sodium chloride.

30% of second material is mixed with first material, charged into a furnace, which is heated to 700 C. and chlorine gas containing 20% of carbon mono-oxide is passed through. The percentages of the yield are as follows: Anhydrous magnesium chloride 81. 5% Sodium chloride 16. 0% Calcium chloride 1. 5% Iron trace.

Water insoluble matter Example IV First material Water insoluble matter -1. 3 Second material: sodium sulphide. i

In the examples shown, it is easily. yerified by experiment that one can obtain sumlar results under the heating temperature in the range of 400 to 800 C. a

Although pure magnesium sulphide which does not contain or is mixed with magnesium oxide is hardly obtained in industrial prodnot, this of course can be treated in quite the same manner as the first materials shown in the examples.

o claim:

1. A process of producing anhydrous magnesium chloride. containing a chloride of alkali metals or of alkaline earth metals; consisting in. mixing magnesium sulphide with chloride of alkali metals, charging the mixture into a furnace, heating the mixture from 400 to 600 C., and passingchlorine gas therethrough While continuing the heatmg.

2. A process of producing anhydrous magnesium chloride containing chloride of alkali metals, consisting in mixing magnesium sulphide with sulphide of alkali metals, charging the mixture into a furnace, heating the mixture from 400 to 600 C., and passing chlorine gas therethrough while continuing the heating.

20 gramsof second material is added toad 8. A process of producing anhydrous mag- 100 grams of first material. By the same nesium chloride contaming chloride of alkaline earth metals, consisting in mixing magnesium sulphide with chloride of alkaline earth metals, charging the mixture into a furnace, heating the mixture from 400 to 600 0., and passing chlorine gas therethrough while continuing the heating,

4. A process of producing anhydrous magnesium chloride contalning chloride of alka line earth metals, consisting in mixing magnesium sulphide with sulphide of alkaline earth metals, charging the mixture into a furnace, heating the mixture from 400 to 600 0., and passing chlorine gas therethrough while continuing the heating.

5. A process of producing anhydrous magnesium chloride containing chloride of alkali metals consisting in mixing magnesium sulphide with chloride of alkali metals, charging the mixture into a furnace, heating the mixture from 400 to 600 0., and passing a reducing gas containing chloride gas therethrough while continuing the heat- 6. A process of producing anhydrous magnesium chloride containing chloride of alkali metals, consisting in mixing magnesium sulphide containing magnesium oxide, with sulphide of alkali metals, charging the mixture into a furnace, heating the mixture from 400 to 600 0., and passing a reducing gas containing chlorine gas therethrough while continuing the heating.

7. A process of producing anhydrous magnesium chloride containing chloride of alka-. line earth metals, consisting in mixing magnesium sulphide containing magnesium oxide, with chloride of alkaline earth metals, charging the mixture into a furnace, heating the mixture from 400 to 600 0., and

passing a reducing gas containing chlorine gas therethrough while continuing the heat- 1n A process of producing anhydrous magnesium chloride containing chloride of alkaline earth metals, consisting in mixing magnesium sulphide containing magnesium oxide, with sulphide of alkaline earth metals, charging the mixture into a furnace, heating the mixture from 400 to 600 0., and passing a reducing gas containing chlorine gas therethrough while continuing the heating.

In testimony whereof they aflix their signatures.

HIROSHI TANAKA. SHOICHIRO IMATOMI. 

